Continuous Solvothermal Synthesis of Metal-Organic Framework (Cu-BTC) Nanoparticles Using a Microstructured Mixer Equipped with Double-Tube, Swirl, and Contraction Flow Channels

Figures & data

Figure 1. Schematic of the experimental setup for continuous Cu-BTC synthesis.

Figure 2. Detailed structure of the microstructured mixer: (a) overall structure; (b) vertical cross-section along the green line; (c) horizontal cross-section along the white line; (d) tip view of tube 2; (e) tip view of the rod; (f) upper end view of tube 3; and (g) lower end view of tube 3.

Table 1. Experimental conditions for continuous Cu-BTC synthesis.

Run	Temperature [K]	Total flow rate [mL/min]	Residence time [s]	Inner fluid	Outer fluid	High-temperature fluid
1	283	100	0.86	Cu(NO3)2	BTC	Ethanol
2	323	100	0.83	Cu(NO3)2	BTC	Ethanol
3	373	100	0.79	Cu(NO3)2	BTC	Ethanol
4	423	100	0.73	Cu(NO3)2	BTC	Ethanol
5	473	100	0.64	Cu(NO3)2	BTC	Ethanol
6	523	100	0.49	Cu(NO3)2	BTC	Ethanol
7	523	25	1.96	Cu(NO3)2	BTC	Ethanol
8	523	100	0.49	Cu(NO3)2	–	BTC
9	523	100	0.49	Cu(NO3)2	Ethanol	BTC
10	523	100	0.49	Cu(NO3)2 + BTC	–	Ethanol
11	523	100	0.49	Cu(NO3)2 + BTC	Ethanol	Ethanol

Figure 3. X-ray diffraction patterns of the products synthesized using the microstructured mixer.

Figure 4. Product yield at each temperature.

Figure 5. Average particle diameter and crystallite diameter of the products at each temperature.

Figure 6. Typical SEM images of the products synthesized using the microstructured mixer.

Figure 7. Particle diameter distribution of the products synthesized at 523 K.